REAGENTS PREPARATION:

1.) Limestone
a. 1:19 HCl= 50mL HCl+ 950mL H2O
b. 1:1 HCl= 500mL HCl+ 500mL H2O
c. 20% NH4Cl (1.53g/cm3)= 13.07g NH4Cl in 100mL H2O
d. Saturated NH4C2O4= 45g NH4C2O4 in 1L H2O
e. 0.05M H2C2O4(90.036g/mol)= 4.5g H2C2O4 in 1L H2O
f. 10% (NH4)2PO4= 250g (NH4)2PO4 in 1L H2O
g. H2SO4 (1+4)= 200mL H2SO4 + 800 mL H2O
h. NH4OH
i. HF
j. H2SO4
k. 0.1 N KMnO4
1.58g H2C2O4 in 250mL H2O= 0.05M H2C2O4
109.9mL H2SO4in 1L H2O= 2M H2SO4
3.3g KMnO4 in 1L H2O→heat for 2 hrs. Stand for 24 hrs. filter

Standardization:

20mL 0.05M H2C2O4+ 20mL 2M H2SO4→ heat to 80ºC. Titrate w/ KMnO4 to permanent pink

Reaction:

2 KMnO4+ 5 (COOH)2+ 3 H2SO4→10 CO2+2 MnSO4+ K2SO4+ 8H2O

Sample Calculation:

Given that 13.68 mL KMNO4 was used in titration to endpoint

20mL (1L/1000mL) (0.05mol H2C2O4/1L) (2mol KMnO4/ 5 mol H2C2O4) =0.04mol KMnO4

0.04mol KMnO4/13.68mL (1000mL/1L)= 0.0292M (5)=0.146N KMnO4

l. MethylRed
0.1g Na salt in100mL H2O or in 30 mL alcohol, dilute to 100mL H2O (pH=4.4-6.2; color
change= red to yellow orange)

2.) Lube Oil

a. P-naphtholbenzein= P-naphtholbenzein + 100mL titration solvent

b. Titration solvent= 500mL toluene+ 495mL isopropyl+ 5mL H2O (100:1:99)

c. 0.1M KOH=6g KOH+1L Isopropyl alc.> boil gently for 10-15 mins. w/ stirring+2g BaOH> boil
gently for 5-10 mins. > Cool to room temp. Stand for several hours, filter supernatant liquid

Standardization:
 0.2g KHP( dired for 1 hr @110+1ºc) + 40mL H2O>titrate to permanent pink w/
phenolphthalein indicator

Calculation:

Normality=Wp/204.23 (1000/ (V-Vb))

Where:

Wp=weight of potassium acid phthalate, g.

204.23= molecular weight of the potassium acid phthalate

V= volume of titrant used to titrate the salt to the specific end point, mL

Vb= volume of titrant used to titrate the blank, mL

3.) H2O Effluent

a. 0.025N (0.004167M ) K2Cr2O7= 1.225g K2Cr2O7( dried at 150ºC for 2 hrs.) in 1L H2O

b. 18M H2SO4= 1L H2SO4+ 0.1g Ag2SO4

c. Ferroin indicator= 1.485g 1,10-phenanthroline monohydrate + 0.695g FeSO4.7 H2O in

100mL H2O

d. 0.025M FAS= dissolve 9.8g Fe (NH4)2 (SO4)2.6 H2O in H2O + 20mL concentrated H2SO4
dilute to 1000mL

e. KHP= 0.425g KHP (dried @ 110ºC) in 1L H2O

Standardization:

10mL K2Cr2O7 to 100mL H2O + 30mL conc. H2SO4. Cool→2-3 drops Ferroin indicator; titrate
with FAS (endpoint: red)

Calculation:

Molarity of FAS= (volume of K2Cr2O7, mL/volume of FAS used in titration, mL) (0.2500)

4.) BOD

a. Phosphate buffer= 8.5g KH2PO4, 21.75g K2HPO4,33.4g NA2HPO4.7 H2O, 1.7g NH4Cl in
500mL H2O→dilute to 1000mL (pH=7.2)

b. Magnesium Sulfate Solution = 22.5g MgSO4.7 H2O in 1L H2O

c. Calcium Chloride= 27.5g CaCl2 in 1L H2O

d. Ferric Chloride= 0.25g FeCl.6 H2O in 1L H2O

e. Acid & Alkali= 28mL conc. H2SO4 in 1L H2O; 40g NaOH in 1L H2O